CN102683168B - A kind of method preparing magnetic germanium quantum point - Google Patents
A kind of method preparing magnetic germanium quantum point Download PDFInfo
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- CN102683168B CN102683168B CN201110327332.7A CN201110327332A CN102683168B CN 102683168 B CN102683168 B CN 102683168B CN 201110327332 A CN201110327332 A CN 201110327332A CN 102683168 B CN102683168 B CN 102683168B
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- quantum point
- germanium
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Abstract
The invention discloses a kind of method preparing magnetic germanium quantum point, first applied chemistry CVD (Chemical Vapor Deposition) method deposit Germanium quantum dot on silicon chip, then apply magnetically controlled sputter method and carry out the in-situ doped of germanium quantum point.In germanium quantum point growth course, magnetic control sputtering system does not work, and after germanium quantum point is formed, utilizes the in-situ doped Mn ion of magnetron sputtering technique.The Ge:Mn magnetic quantum dot applying this chemical gaseous phase-sputtering method growth is low to be equably dispersed on silicon chip, in spherical form that is beautiful, high degree of symmetry, and at room temperature there is very strong saturation magnetization and coercive force, present very strong ferromagnetism feature.This magnetic Ge:Mn quantum dot can be used for preparing various electromagnetic diode, electromagnetism triode and field-effect transistor etc.
Description
Technical field
The present invention relates to semiconductor applications, be specifically related to a kind of method preparing magnetic germanium quantum point.
Background technology
In recent years, mix magnetic particle in the semiconductors, make the electronics in semiconductor not only have the charge characteristic of electronics, be also provided with spin properties, this semiconductor is called dilute magnetic semiconductor.Semiconductor Germanium, owing to having higher Curie temperature, makes its rare magnetic characteristic cause the research interest of people.Higher Curie temperature is very important to preparing germanium base electromagnetic device.Because semiconductor Germanium and Si ic manufacturing technology have very high compatibility, people are made to be easy to utilize Si technology to manufacture electronics and the magnetic memory device of various advanced person.
Now, be all studied much about the structure of germanium single crystal, nano wire etc. of Mn doping and electromagnetic property.Ge has been prepared as the people such as Park apply molecular beam epitaxial method (MBE)
1-xmn
xalkene magnetic thin film, finds that its Curie temperature (Curie temperature, CT) changes within the scope of 25-116K, and with the increase of Mn content, Curie temperature increases thereupon.Subsequently, the people such as S.Cho reports the Curie temperature of the Ge monocrystalline of Mn doping up to 285K.The Ge of D.Holmes seminar synthesis
1-xmn
xferromagnetism temperature at 300K.In these researchs, be all the rare magnetic characteristic that have studied the monocrystalline of Ge, film and nano wire substantially, and for the also not relevant at home report of the research of the rare magnetic characteristic of germanium quantum point.Also molecular beam epitaxial method is mainly utilized to prepare germanium quantum point, this apparatus expensive, technical sophistication abroad.A kind of simple technique preparing germanium magnetic quantum dot of this patent Introduction, and analyze its magnetic mechanism.
Summary of the invention
The object of the present invention is to provide a kind of method preparing magnetic germanium quantum point, is a kind of straightforward procedure of in-situ doped germanium quantum point.
A kind of method preparing magnetic germanium quantum point of the present invention, concrete preparation method is as follows:
Step 1) uses the reactive magnetic control sputtering system be made up of this six part of settling chamber, extract system, heating system, gas Flowrate Control System, plasma rf system and magnetic control sputtering system as growing system;
Step 2) select n-type silicon chip (100 crystal face) as substrate, use acetone, ethanol, deionized water Ultrasonic Cleaning successively, then dry up with nitrogen, put the centre of negative electrode in the plasma rf system in growing system into;
Step 3) adopt germane (purity is 99.9999%) as reacting gas, argon gas as dilution and sputter gas, manganese target (purity is 99.9999%) doping target;
Step 4) first applied chemistry vapour deposition deposit Germanium quantum dot, then applies magnetically controlled sputter method and carries out the in-situ doped of germanium quantum point, obtain magnetic germanium quantum point.Concrete operations are:
Pass into germane and argon gas, the reaction ratio of germane and argon gas two kinds of gases is 1:19, and under plasma rf effect, germane is decomposed into germanium atom, H
+, hydrogen atom, reaction pressure be 40Pa-60Pa, growth temperature be the condition of 450 DEG C-550 DEG C under germanium atom deposit on silicon chip and form germanium strained quantum point, the growth time of germanium quantum point is 0.5-1.5 hour;
Then on germanium strained quantum point, the doping of manganese is carried out: open magnetic control sputtering system, manganese target is aimed at germanium strained quantum point surface and evenly mix manganese, adulterate and at the temperature of 550 DEG C-650 DEG C, carry out hot short annealing 35-45 minute after 8-12 minute;
Measured the concentration of manganese in accurate germanium strained quantum point again by Lu Saifu back scattering, reach 10
15cm
-3.
Preferably, in the concrete operations of step 4), be at reaction pressure 50Pa, under growth temperature 500 DEG C of conditions, germanium atom deposits on silicon chip and forms germanium atom strained quantum point, and the growth time of germanium quantum point is 1 hour.
Preferably, in the concrete operations of step 4), be manganese target is aimed at germanium strained quantum point surface evenly to mix manganese, adulterate and at 600 DEG C of temperature, carry out hot short annealing 40 minutes after 10 minutes.
Beneficial effect: preparation method of the present invention, utilizes chemical gaseous phase depositing process to grow and in-situ doped Mn, 600 DEG C of rear obtained magnetic germanium quantum points of annealing.Find that applied chemistry gas phase-sputtering method Ge:Mn quantum dot is spherical form that is beautiful, high degree of symmetry by atomic force microscope observation, to be evenly lowly dispersed on silicon chip.And the surface of germanium quantum point is very even, smooth, does not stick other impurity or the generation of other defect, and there is the very strong magnetic characteristic of iron.
Accompanying drawing explanation
Fig. 1 is the experimental provision schematic diagram preparing additive Mn germanium quantum point of the present invention.
Fig. 2 is the X-ray diffractogram of additive Mn germanium quantum point of the present invention.
Fig. 3 is the energy dispersive spectrum of additive Mn germanium quantum point of the present invention.
Fig. 4 is the graceful spectrogram of receiving of additive Mn germanium quantum point of the present invention.
Fig. 5 be under additive Mn germanium quantum point sample room temperature of the present invention magnetic susceptibility with the variation relation figure of magnetic field intensity.
The magnetic susceptibility schematic diagram of Fig. 6 additive Mn germanium quantum point of the present invention sample.
The magnetic moment Peff schematic diagram of each Mn in Fig. 7 additive Mn of the present invention germanium quantum point.
Embodiment
A kind of method preparing magnetic germanium quantum point of the present invention, concrete preparation method is as follows:
Prepare the experimental provision of manganese (Mn) doped germanium quantum dot as Fig. 1, use growing system used for reactive magnetic control sputtering system, be made up of this six part of settling chamber, extract system, heating system, gas Flowrate Control System, plasma rf system and magnetic control sputtering system.
Select n-type silicon chip (100 crystal face) as substrate, use acetone, ethanol, deionized water Ultrasonic Cleaning successively, then dry up with nitrogen, put the centre of the negative electrode of settling chamber's plasma into.Adopt high-purity germane GeH4(purity 99.9999%) as reacting gas, argon gas (Ar) is as dilution and sputter gas.High-purity manganese target (purity 99.9999%) is as doping target.
The experiment of additive Mn germanium quantum point is divided into two steps: first applied chemistry vapour deposition deposit Germanium quantum dot, then applies magnetically controlled sputter method and carries out the in-situ doped of germanium quantum point.In germanium quantum point growth course, magnetic control sputtering system does not work, and rotary sputtering target makes it depart from sample direction.Pass into germane and argon gas, two kinds of gas reaction ratios are 1:19.Under plasma rf effect, GeH4 is decomposed into Ge atom, H
+, hydrogen atom, at reaction pressure 50Pa, under growth temperature 500 DEG C of conditions, germanium atom deposits on silicon chip and forms Ge strained quantum point.Germanium quantum point growth time is 1 hour.In Mn doping process, open magnetic control sputtering system, high-purity manganese target is aimed at sample surfaces and evenly mixes Mn.Adulterate and at 600 DEG C of temperature, carry out hot short annealing 40 minutes (RTA) after 10 minutes.Then, measured the concentration of Mn in sample by Lu Saifu back scattering (RBS), reach 10
15cm
-3.After doping terminates, take out sample after waiting reative cell cool to room temperature, carry out the measurement of structure, composition and magnetic characteristic.
The surface topography of the germanium quantum point sample of deposition is observed by atomic force microscope (AFM); X-ray diffraction (XRD) (RINT2000, Cu K
αbeam wavelength λ=0.1541nm) analyze the architectural characteristic of germanium quantum point, applied energy scattering spectra and the Lu Saifu backscattering analysis doping content of Mn.Finally, the magnetism characteristic that superconducting quantum interference device (SQUID) (SQUID) measures germanium quantum point is applied.
Chemical gaseous phase depositing process is utilized to grow and in-situ doped Mn, the surface topography map of germanium quantum point after 600 DEG C of annealing and graphics as can be seen from what observe, the germanium quantum point of even-grained circle is dispersed on silicon chip, applied chemistry gas phase-sputtering method Ge:Mn quantum dot is spherical form that is beautiful, high degree of symmetry, is evenly lowly dispersed on silicon chip.The surface of germanium quantum point is also very even, smooth, does not stick other impurity or the generation of other defect.The average height of quantum dot is 8nm, diameter range 20-60nm, and the density of quantum dot is 1.1 × 10
13cm
-2.
Fig. 2 is the X-ray diffractogram of Mn doped germanium quantum dot.Can see, 3 very strong diffraction maximums, lay respectively at 27.45 °, 45.51 °, 53.88 °, respectively (111), (220) and (311) crystal face of corresponding Ge.Mn5Ge3 phase or other mutually secondary ferromagnetic alloy is there is not mutually in X-ray diffraction peak.Illustrate and carry out adulterating with the position of replacing Ge atom after Mn mixes germanium quantum point, do not destroy the structure of germanium.Show further, the magnetic germanium quantum point utilizing chemical vapor in-situ method to grow has very high quality.
Fig. 3 is the energy dispersive spectrum of Mn doped germanium quantum dot.Only containing the peak from Ge, Si and Mn atom in power spectrum, normalized percentage is respectively 48%, 37.6% and 6.4%.Si is mainly from the silicon of substrate, and the appearance at Mn peak illustrates that Mn atom is mixed with in germanium quantum point effectively, and ratio shared in germanium quantum point is 6.4%.Thus, what we can infer germanium quantum point sample consists of Ge0.88Mn0.12.
Fig. 4 is the graceful spectrum of receiving of magnetic germanium quantum point, can find out, germanium quantum point to receive the intensity of Man Feng very strong, shape is more symmetrical, illustrates that this quantum dot has good crystallinity.The feature of Ge is received Man Feng and is positioned at 280cm
-1, the Man Feng that receives of germanium quantum point is positioned at 298cm
-1, move 18cm to long wave number direction
-1. this is because the limit threshold effect of quantum dot causes.
Fig. 5 is the magnetism characteristic of the magnetic germanium quantum point that under room temperature, (300K) measures.Can find out, with the increase in magnetic field, the magnetization significantly increases.When magnetic field reaches H2500 Oe, the magnetization reaches capacity value 2.2 × 10
-4emu/g.Subsequently, with the reduction in magnetic field, the magnetization slowly reduces.Reduce speed be obviously less than climbing speed, this just make when magnetic field less to 0 time, the magnetization is also non-vanishing, but has certain remanent magnetism, and this remanent magnetism is 0.24 × 10
-4emu/g; And when adding opposing magnetic field and reaching 193 Oe, the magnetization is just reduced to zero completely, this just illustrates that the coercive force of germanium quantum point sample is 193 Oe.When continuation increases opposing magnetic field, obtain and very symmetrical curve under forward magnetic field conditions.Wide, a level and smooth magnetic hysteresis loop is formed with forward magnetic field.This magnetic hysteresis loop is the symbolic characteristic curve of magnetic material.Remanent magnetism and coercive force are then the notable features of ferrimagnet.Illustrate that the magnetic germanium quantum point that we deposit has the very strong magnetic characteristic of iron.
Fig. 6 is the magnetic susceptibility schematic diagram of Mn doped germanium quantum dot sample, and its maximum magnetic susceptibility is 0.04 × 10
-6.The Effect magnetic moment P of each Mn atom
efffor saturation magnetization Ms is divided by total manganese atom number N
mn, i.e. P
eff=M
s/ N
mn.According to Lu Saifu back scattering, the doping content of Mn atom in germanium quantum point is 10
15cm
-3, then each Effect magnetic moment of manganese atom and the relation of externally-applied magnetic field can be obtained according to the magnetization surveyed.As Fig. 7, can find out, the maximum Effect magnetic moment of each manganese atom is 2.36 μ
b, μ
bfor Bohr magneton, μ
b=9.274 × 10
-21erg.G
-1.Effect magnetic moment 0.7 μ of the Ge nano wire of the Mn doping that this value is reported much larger than J.D.Holmes and H.J.Choi groups
b(300K) He 0.87 μ
b(5K).
The increase of this Effect magnetic moment mainly produces due to the minimum wavelength threshold effect of Ge quantum dot and the exchange interaction pattern of Mn atom.The atomic configuration of Mn atom is 3d
54s
2, 5d track has a large amount of rooms, and mainly based on hole conduction (p-type semiconductor), then, the doping content of our sample is 10 to this Ge quantum dot just causing Mn to adulterate
15cm
-3, hole concentration is too low is not enough to the ferromagnetism feature that formation take hole as medium.Because Mn atom also has hole this ferromagnetism of many constraints RKKY(Ruderman-Kittel-Kasuya-Yosida effectively certainly) to exchange mutual effect relevant.KRRY coupling is a kind of indirect mutual effect by free hole charge carrier.Hole produces a kind of exchange coupling freely, and the localized holes of constraint is polarized.The spin of localized holes can make ambient magnetic impurity polarize, Here it is so-called bonding state magnetic polaron.Polarize in system is all the hole that fetters for medium carries out mutual effect.Therefore, the interionic RKKY coupling of Mn is all medium with hole, the Exchange Coupling of hole in the hole of bound state and contiguous Mn between bound state hole plays very important effect, the exchange coupling of Mn ion in Ge quantum dot is strengthened, thus the Effect magnetic moment of each Mn ion is increased.
By the doping of Mn, obtain the germanium quantum with strong ferromagnetic characteristics.This magnetic quantum dot can be used for preparing the free electronic device of various germanium quantum point.
Above-described embodiment, just in order to technical conceive of the present invention and feature are described, its objective is and is one of ordinary skilled in the art can be understood content of the present invention and implement according to this, can not limit the scope of the invention with this.The change of every equivalence done by the essence of content of the present invention or modification, all should be encompassed in protection scope of the present invention.
Claims (7)
1. prepare a method for magnetic germanium quantum point, it is characterized in that, concrete preparation method is as follows:
Step 1) uses the reactive magnetic control sputtering system be made up of settling chamber, extract system, heating system, gas Flowrate Control System, plasma rf system and magnetic control sputtering system six part as growing system;
Step 2) select n type silicon chip as substrate, use acetone, ethanol, deionized water Ultrasonic Cleaning successively, then dry up with nitrogen, put the centre of negative electrode in the plasma rf system in growing system into;
Step 3) adopts germane as reacting gas, and argon gas is as dilution and sputter gas, and manganese target is as doping target;
Step 4) first applied chemistry vapour deposition deposit Germanium quantum dot, then applies magnetically controlled sputter method and carries out the in-situ doped of germanium quantum point, obtain magnetic germanium quantum point.
2., according to the method preparing magnetic germanium quantum point described in claim 1, it is characterized in that, step 2) described in n-type silicon chip be 100 crystal faces.
3. the method preparing magnetic germanium quantum point according to claim 1, is characterized in that, step 2) described in the purity of germane be 99.9999%, the purity of manganese target is 99.9999%.
4. according to the method preparing magnetic germanium quantum point described in claim 1, it is characterized in that, the concrete operations of described step 4) are:
Germanium quantum point growing method: pass into germane and argon gas, under plasma rf effect, germane is decomposed into germanium atom, H
+, hydrogen atom, reaction pressure be 40Pa-60Pa, growth temperature be the condition of 450 DEG C-550 DEG C under germanium atom deposit on silicon chip and form germanium strained quantum point, the growth time of germanium quantum point is 0.5-1.5 hour; Then on germanium quantum point, the doping of manganese is carried out: open magnetic control sputtering system, manganese target is aimed at germanium strained quantum point surface and evenly mix manganese, adulterate and at the temperature of 550 DEG C-650 DEG C, carry out hot short annealing 35-45 minute after 8-12 minute; Measured the concentration of manganese in germanium quantum point again by Lu Saifu back scattering, reach 10
15cm
-3.
5. according to the method preparing magnetic germanium quantum point described in claim 4, it is characterized in that, in the concrete operations of step 4), the reaction ratio passing into germane and argon gas two kinds of gases is 1: 19.
6. according to the method preparing magnetic germanium quantum point described in claim 4, it is characterized in that, in the concrete operations of step 4), at reaction pressure 50Pa, under growth temperature 500 DEG C of conditions, germanium atom deposits on silicon chip and forms germanium strained quantum point, and the growth time of germanium quantum point is 1 hour.
7. according to the method preparing magnetic germanium quantum point described in claim 4, it is characterized in that, in the concrete operations of step 4), be manganese target is aimed at germanium strained quantum point surface evenly to mix manganese, adulterate and at 600 DEG C of temperature, carry out hot short annealing 40 minutes after 10 minutes.
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| CN108004518A (en) * | 2017-10-17 | 2018-05-08 | 云南大学 | Size uniform, high density MnGe quantum dots are prepared based on ion beam sputtering technology |
| CN114427114B (en) * | 2022-01-25 | 2022-11-11 | 云南大学 | Manganese-tellurium-doped germanium quantum dot and preparation method and application thereof |
| CN114752887B (en) * | 2022-05-20 | 2023-10-20 | 云南大学 | Method for preparing MnGe ferromagnetic quantum dot material by utilizing magnetron co-sputtering technology |
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| CN101431014A (en) * | 2008-12-18 | 2009-05-13 | 绍兴文理学院 | Production method for Ge/Si quantum ring electric charge storing device |
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Non-Patent Citations (2)
| Title |
|---|
| Ferromagnetism in Mn-Implanted Epitaxially Grown Ge on Si(100);S. Guchhait，et al;《Physical Review B》;20110729;第84卷(第2期);第024432-1~024432-8页 * |
| Ferromagnetism of Mn5Ge3 Precipitates in Mn-implanted Self-organized Ge/Si Quantum Dots;I.T. Yoon;《J Supercond Nov Magn》;20090919;第23卷(第3期);第319-323页 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9864138B2 (en) | 2015-01-05 | 2018-01-09 | The Research Foundation For The State University Of New York | Integrated photonics including germanium |
| US10295745B2 (en) | 2015-01-05 | 2019-05-21 | The Research Foundation For The State University Of New York | Integrated photonics including germanium |
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